반응 #481920

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7-fluoro-4-[(3-methyl-phenyl)amino]-6-nitroquinazoline

MeOH CH2Cl2 EtOAc

3-morpholinopropan-1-ol

sodium

→

4-[(3-methylphenyl)-amino]-7-[(3-morpholino)propyloxy]-6-nitroquinazoline

수율 88.0%

용매

THF

CH2Cl2 hexane

EtOAc

MeOH

THF

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후처리

1. 1
   기타The reaction procedure and workup

실험 절차

To a solution of 3-morpholinopropan-1-ol (8.40 mmol, 1.22 g) in THF (40 mL) under N2 was added sodium metal (11.8 mmol, 0.27 g). The resulting suspension was stirred at 20° C. for 2 hours and then cannulated into a solution of 7-fluoro-4-[(3-methyl-phenyl)amino]-6-nitroquinazoline (0.70 g, 2.35 mmol) in THF (30 mL) under N2. The reaction procedure and workup above were followed to give after chromatography on silica gel eluting with MeOH/CH2Cl2/EtOAc (5:45:50) to MeOH/CH2C0.50/EtOAc (3:7:10) 4-[(3-methylphenyl)-amino]-7-[(3-morpholino)propyloxy]-6-nitroquinazoline (0.87 g, 88%) as a yellow powder, mp (CH2Cl2/hexane) 169-170° C.

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